JP2014515720A5

JP2014515720A5 -

Info

Publication number: JP2014515720A5
Application number: JP2013558343A
Authority: JP
Filing date: 2012-02-03
Publication date: 2015-07-23
Anticipated expiration: 2032-02-03

Description

本発明のさらなる対象は、本発明によるケイ素−アルミニウム混合酸化物粉末の製造方法であって、
ａ）ＣＨ₃ＳｉＣｌ₃、（ＣＨ₃）₂ＳｉＣｌ₂、（ＣＨ₃）₃ＳｉＣｌおよび（ｎ−Ｃ₃Ｈ₇）ＳｉＣｌ₃からなる群から選択される１つまたは複数のケイ素化合物を含んでいる蒸気、ならびに加水分解可能およびは酸化可能のアルミニウム化合物の蒸気を、別個または一緒に、キャリアガスを用いて混合室に移し、ここで、アルミニウム化合物（Ａｌ₂Ｏ₃として算出）のケイ素化合物（ＳｉＯ₂として算出）に対する質量比は０．００３〜０．０５であり、
ｂ）それとは別に、少なくとも１つの燃料ガスおよび空気を前記混合室に移し、ここで、空気中の酸素の総量は、燃料ガスならびにケイ素化合物およびアルミニウム化合物を完全に燃焼させるために少なくとも充分であり、
ｃ）前記ケイ素化合物およびアルミニウム化合物の蒸気、燃料ガスおよび空気からの混合物を燃焼装置内で点火して、この火炎を反応室内に入れて燃焼させ、
ｄ）引き続き前記固体をガス状物質から分離し、その後この固体を水蒸気で処理する、
前記方法である。 A further subject of the present invention is a process for producing a silicon-aluminum mixed oxide powder according to the invention,
a) including one or more silicon compounds selected from the group consisting of CH ₃ SiCl ₃ , (CH ₃ ) ₂ SiCl ₂ , (CH ₃ ) ₃ SiCl and (n-C ₃ H ₇ ) SiCl ₃ Vapor and vapors of hydrolyzable and oxidizable aluminum compounds are transferred, separately or together, to the mixing chamber using a carrier gas, where silicon compounds (SiO ₂ ) of aluminum compounds (calculated as Al ₂ O ₃ ) _The mass ratio to (calculated as ₂ ) is 0.003 to 0.05,
b) Alternatively, at least one fuel gas and air is transferred to the mixing chamber, wherein the total amount of oxygen in the air is at least sufficient to completely combust the fuel gas and silicon compound and an aluminum compound And
c) vapor of the silicon compound and aluminum compound, and ignites the mixture from fuel gas and air in the combustion device, is burned to put the flame into the reaction chamber,
d) subsequently separating the solid from the gaseous substance and then treating the solid with steam;
Said method.

前記方法は、ケイ素化合物の蒸気がＳｉＣｌ₄を４０質量％まで含んでいてよいように実施することもできる。特に好ましくは、ＣＨ₃ＳｉＣｌ₃ ６５〜８０質量％とＳｉＣｌ₄ ２０〜３５質量％とからの混合物であってよい。アルミニウム化合物として、好ましくは塩化アルミニウムが好適である。前記燃料ガスは、水素、メタン、エタン、プロパンおよびそれらの混合物からなる群から選択されるのが好ましい。特に好ましいのは、水素である。前記混合室に導入された空気は、少なくとも前記燃料ガスおよびケイ素化合物およびアルミニウム化合物を完全に燃焼させるに充分である。通常、過剰の空気が使用される。水蒸気での処理は、粒子に付着した塩化物残留物を可能な限り除去する目的のために用いられ、その結果、前記粉末は、塩化物を１質量％以下、好ましくは塩化物を０．２質量％以下含んでいる。 The method can also be carried out such that the silicon compound vapor may contain up to 40% by weight of SiCl ₄ . Particularly preferably, it may be a mixture of 65 to 80% by mass of CH ₃ SiCl ₃ and 20 to 35% by mass of SiCl ₄ . As the aluminum compound, aluminum chloride is preferable. The fuel gas is hydrogen, methane, ethane, be selected from the group consisting of propane and mixtures thereof. Particularly preferred is hydrogen. The air introduced into the mixing chamber is sufficient to completely burn at least the fuel gas and the silicon compound and aluminum compound. Usually excess air is used. The treatment with water vapor is used for the purpose of removing as much as possible chloride residue adhering to the particles, so that the powder contains less than 1% by weight of chloride, preferably 0.2% of chloride. Contains less than mass%.

Claims

A majority or all of a silicon-aluminum mixed oxide powder present in the form of agglomerated primary particles,
a. The mass ratio (Al ₂ O ₃ / SiO ₂ ) _{ttl in the} whole primary particles is 0.003 to 0.05,
b. The primary particle mass ratio (Al ₂ O ₃ / SiO ₂ ) surface in a layer close to a 5 nm thick _surface is smaller than in the entire primary particle, and c. The BET surface area is 50-250 m ² / g,
The mixed oxide powder characterized by the above.

_2. The silicon-aluminum mixed oxide powder according to claim 1, wherein the _{surface of} (Al ₂ O ₃ / SiO ₂ ) _ttl / (Al ₂ O ₃ / SiO ₂ ) is 1.3 to 20. ₃ .

3. The silicon-aluminum mixed oxide powder according to claim 1, wherein the number of dibutyl phthalates represented by g of dibutyl phthalate / 100 g of mixed oxide is 300 to 350. 4.

In the manufacturing method of the silicon-aluminum mixed oxide powder according to any one of claims 1 to 3,
a) including one or more silicon compounds selected from the group consisting of CH ₃ SiCl ₃ , (CH ₃ ) ₂ SiCl ₂ , (CH ₃ ) ₃ SiCl and (n-C ₃ H ₇ ) SiCl ₃ Vapor and vapors of the hydrolyzable and / or oxidizable aluminum compound are transferred separately or together to the mixing chamber using a carrier gas, where SiO ₂ of the aluminum compound calculated as Al ₂ O ₃ The mass ratio to the silicon compound calculated as is 0.003 to 0.05,
b) separately from the transferred at least one fuel gas and air into the mixing chamber, wherein the total amount of oxygen in the air, at least in order to completely burn fuel gas and silicon compound and an aluminum compound Enough,
c) vapor of the silicon compound and aluminum compound, and ignites the mixture from fuel gas and air in the combustion device, is combusted placed in the reaction chamber to the flame,
d) subsequently separating the solid from the gaseous substance and then treating the solid with steam;
Said method.

Vapor of the silicon compound, characterized in that it contains SiCl ₄ to 40 wt%, The method of claim 4.

Use of the silicon-aluminum mixed oxide powder according to any one of claims 1 to 3 as a catalyst.